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है”ह”ह

IS 11255-7 (2005): Methods for measurement of emission fromstationary sources, Part 7: Oxides of nitrogen [CHD 32:Environmental Protection and Waste Management]

IS 11255 (Part 7) :2005

m731@il=lhifmm@

Indian Standard

METHODS FOR MEASUREMENT OF EMISSIONFROM STATIONARY SOURCES

PART 7 OXIDES OF NITROGEN

Ics 13.040.40

0 BIS 2005

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

,Tepteinber 2005 Price Group 3

Environment Protection and Waste Management Sectional Committee, CHD 32

FOREWORD

This Indian Standard (Part 7) was adopted by the Bureau of Indian Standards after the dratl finalized by theEnvironment Protection and Waste Management Sectional Committee had been approved by the Chemical DivisionCouncil.

Nitrogen oxides (NOX)the term is used to describe the total NO, NOZand other oxides of nitrogen are consideredimportant due to their role in the formation of ozone (a secondary air pollutant) through a complex series ofpetrochemical reactions involving volatile organic compounds. NO, are emitted as part of most fuel combustionprocess, with nitric oxide (NO) being a primary constituent. The majority (95 percent) of nationwide NO, that isproduced from fuel combustion sources is NO with the remaining fraction being predominantly N02.

Exposure to nitrogen dioxide occurs; through the pulmonary system. NOZ irritates the lungs. Asthmatics aremore sensitive to the effect of N02 than the general population. Exercise increases the ventilation rate and henceexposure to NO1. Some studies have shown a relationship between indoor NOZexposures and increased respiratoryillness in young children, short-term NOZexposures (< 3 h duration) at or near ambient concentration levels forsome communities in the United States have resulted in an increased respiratory illness in children between 5 and12 years old, and airway responsiveness/pulmonary function changes in those individuals with pre-existingrespiratory illnesses. Long-term exposure levels have been associated with increased susceptibility to respirato~infections and cause lung alterations.

There is no 1S0 standard on this subject. This standard is developed based on the indigenous technology availablein India.

The composition of the Committee responsible for the formulation of this standard is given at Annex A.

In reporting the result of a test or analysis made in accordance with this standard, if the’final value, observed orcalculated, is to be rounded off, it shall be done in accordance with IS 2: 1960 ‘Rules for rounding off numericalvalues (revised)’.

IS 11255 (Part 7) :2005

Indian Standard

METHODS FOR MEASUREMENT OF EMISSIONFROM STATIONARY SOURCES

PART 7 OXIDES OF NITROGEN

1 SCOPE

This standard (Part 7) prescribes the methods fordetermination of oxides of nitrogen from stationarysources.

2 PRINCIPLE AND APPLICABILITY

2.1 Principle

A grab sample is collected in a dilute sulphuric acid-hydrogen peroxide absorbing solution, and thenitrogen oxides, except nitrous oxide, are measuredcalorimetrically using the phenoldisulphonic acid(PDS) procedure.

2.2 Applicability

This method is applicable to the measurement ofnitrogen oxides emitted from stationary sources. Therange of the method has been determined to be 2 to400 milligrams NOX(as N02) per standard cubic metre,without having to di!ute the sample.

3 APPARATUS

3.1 Sampling Apparatus — The assembled samplingapparatus is shown in Fig. 1. It consists of the-followingparts.

3.1.1 Probe — Borosilicate glass tubing, sufficientlyheated to prevent water condensation and equippedwith an in-stack or out-stack filter to remove particulatematter (a plug of glass wool is satisfactory for thispurpose).

NOTES

1 Stainless steel or Teflon tubing may also be used for theprobe.

2 Heating is not necessary if the probe remains dry during thepurging period.

3.1.2 Collection Flask — Two-litre borosilicate roundbottom flask, with short neck and 24/40 standard taperopening, protected against implosion -or breakage.

3.1.3 Flask Valve — T-bore stopcock connected to a24/40-standard taper joint.

3.1.4 Temperature Gauge — Dial-type thermometer,or other temperature gauge, capable of measuring 1“Cintervals from –5 to 50”C.

3.1.5 Vacuum Line— Tubing capable-of withstandinga vacuum of 75 mm Hg absolute pressure, with ‘T’connection and T-bore stopcock.

3.1.6 Vacuum Gauge — U-tube manometer, 1 m high,with 1 mm divisions, or other gauge capable ofmeasuring pressure to within + 2.5 mm Hg.

3.1.7 Pump — Capable of evacuating the collectionflask to a pressure equal to or less than 75 mm Hgabsolute.

3.1.8 Squeeze Bulb — One way.

3.1.9 Stopcock

3.1.10 Barometer — Mercury, aneroid, or otherbarometer capable of measuring atmospheric pressureto within 2.5 mm Hg.

3.2 Porcelain Evaporating Dishes — 175 to 250 mlcapacity with lip for pouring, one for each sample andeach standard.

3.3 Steam Bath — Low temperature ovens orthermostatically controlledhot plates kept below 70°C.

3.4 Policeman Porcelain — One for each sample andeach standard.

3.5 Graduated Cylinder — 100 ml with 1 mldivisions.

3.6 Spectrophotometer — To measure absorbanceat410nm.

3.7 pH Paper

3.8 Analytical Balance — Accuracy 0..1 mg.

4 REAGENTS

4.1 Absorbing Solution — To prepare the absorbingsolution, cautiously add 2.8 ml concentrated H2SOAto1 Iitre of distiiled water. Mix well and add 6 ml of3 percent hydrogen peroxide, freshly prepared from30 percent hydrogen peroxide solution.

NOTE — The absorbing solution should be used within I weekof its preparation. Do not expose to extreme heat or directsunlight.

4.2 Sodium Hydroxide (1 N) — Dissolve 40 g NaOHin distilled water and dilute to 1 Iitre.

1

IS11255

(Part

7):2005

IIIn

insit

u=4XII-u-)

(naOAZ

.0

,

2

4.3 Fuming Sulphuric Acid, 15 to 18 percent byweight free sulphur trioxide.

NOTE — Highly corrosive, handle with care.

4.4 Phenol, white solid.

4.5 Sulphuric Acid, concentrated 95 percent minimumassay.

NOTE — Highly corrosive, handle with care.

4.6 Potassium Nitrate — Dried at 105° to 11O°C.fora minimum period of 2 h just prior to preparation ofstandard solution.

4.7 Standard -KNO~ Solution — Dissolve 2.198 gdried potassium nitrate (KNOJ in distilled water anddilute to 1 litre with distilled water in a 1000 mlvolumetric flask.

4.8 Working Standard KNOJ Solution — Dilute10 ml of the standaid solution to 100 ml with distilledwater. One millilitre of the working standard solutionis equivalent to 100 pg nitrogen dioxide (NOz).

4.9 Phenoldisulphonic Acid Solution — Dissolve25 g of pure white phenol in 150 ml concentratedsulphuric acid on a steam bath. Cool, add 75 -mlfumingsulphuric acid, and heat at 100”C for 2 h. Store in adark, stoppered bottle.

5 PROCEDURE

5.1 Sampling

5.1.1 Pipette 25 ml of absorbing solution into a sampleflask, retaining a suftlcient quantity for use in preparingthe calibration standards. Insert the flask valve-stopperinto the flask with the valve in the ‘purge’ position.Assemble the sampling train as shown in Fig. 1 andplace the probe at the sampling point. Make sure thatall fittings are tight and leak-free and that all groundglass joints have been properly greased with a highvacuum, high temperature chlorofluorocaibon basedstopcock grease. Turn the flask valve and the pumpvalve to their ‘evacuate’ position. Evacuate the flaskto 75 mm Hg absolute pressure, or less. Evacuationto a pressure approaching the vapour pressure of waterat the existing.temperature is desirable. Turn the pumpvalve to its ‘vent’ position and turnoff the pump. Checkfor leakage by observing the manometer for anypressure fluctuation. Any variation greater than10 mm Hg over a period of 1 minute is not acceptable,and the flask is not to be used until the leakageproblem is corrected. Pressure in the flask is not toexceed 75 mm Hg absolute at the time sampling iscommenced. Record the volume of the flask and valve(Vi), the flask temperature (Ti) and the barometric

fpressure. Turn the flask valve counterclockwise to its‘purge’ position and do the same with the pump valve.

IS 11255 (Part 7) :2005

Purge the probe and the vacuum tube using the squeezebulb. If condensation occurs in the probe and the flaskarea, heat the probe and purge until the condensationdisappears. Next, turn the pump valve to its ‘vent’position. Turn the flask valve clockwise to its‘evacuate’ position and record the difference in themercury levels in the manometer. The absolute internalpressure in the flask (Pi) is equal to the barometricpressure less the mhnometric reading. Immediately turnthe flask valve to the ‘sample’ position and permit thegas to enter the flask until pressures in the flask andsample line (that is duct, stack) are equal. This willusually require about 15 s; a longer period indicates a‘plug’ in the probe, which must be corrected beforesampling is continued. After collecting the sample, turnthe flask valve to its ‘purge’ position and disconnectthe flask from the sampling train. Shake the flask forat least 5 min.

5.1.2 If the gas being sa@rnpledcontains insufficientoxygen for the conversion of NO to N02 then oxygenshall be introduced into the flask by one of thefollowing three methods:

a)

b)

c)

Before evacuating the sampling flask,flush with pure cylinder oxygen, thenevacuate flask to 75 mm Hg absolute pressureless;

Inject oxygen into Ihe flask after sampling;or

Terminate sampling with minimum 50 mm Hgvacuum remaining in flask, record the finalpressure and vent the flask to atmosphere untilthe flask pressure is equal to the atmosphericpressure.

5. L3 Sample Recovery

Let the flask set for a minimum of 16 h and then shakethe contents for 2 min. Connect the flask to mercuryfilled U-tube manometer. Open the valve-from the flaskto the manometer and record the flask temperature (TJ,the barometric pressure, and the difference betweenthe mercury levels in the manometer. The absoluteinternal pressure in the flask (PJ is the barometricpressure less the manometer reading. Transfer thecontents of the flask to a leak-free polyethylene bottle.Rinse the flask twice with 5 ml portions of distilledwater and add the rinse water to the battle. Adjust thepH to between 9 and 12 by adding sodium hydroxide(1 N), dropwise (about 25 to 35 drops). Check the pHby dipping a stirring rod into solution and then touchingto the pH test paper. Remove as little material aspossible during this step. Mark the height of the liquid

3

IS 11255 (Part 7) :2005

level so that the container can be checked for leakageafter transport. Label the container to clearly identifyits contents.

5.2 Analysis

Note the level of the liquid in container and confirmwhether or not any sample was lost during shipment;note this on analytical data sheet. Immediately priorto analysis, transfer the contents of the shippingcontainer to a 50 ml volumetric flask and rinse thecontainer twice with 5 ml portions of distilled water.Add the rinse water to the flask and dilute to the markwith distilled water; mix thoroughly. Pipette a 25 mlaliquot into the porcelain evaporating dish. Return anyunused portion of the sample to the polyethylenestorage bottle. Evaporate the 25 ml aliquot to drynesson a steam bath an-d allow to cool. Add 2 mlphenoldisulphonic acid solution to the dried residue

%sand triturate thoroughly wi,, a polyethylene policeman.Make sure the solution co’ cts all residue. Add 1 mldistilled water and four drops of concentrated sulphuricacid. Heat the solution on a steam bath for 3 min withoccasional stirring. Allow the solution to cool, add20 ml distilled water, mix well by stirring and addconcentrated, ammonium hydroxide, dropwise, withconstant stirring, until the pH is 10 (as determined byPH paper). If the sample contains solids, these shall beremoved by filtration as follows:

Filter through Whatman No. 41 or equivalent into a100 ml volumetric flask, rinse the evaporating dishwith three 5 ml portions of distilled water; filter thesethree rinses.

Wash the filter with at least three 15 ml portions ofdeionized, distilled water. Add the filter washings tothe contents of the volumetric flask and dilute to themark with distilled water. If the solids are absent,transfer the solution directly to the 100-ml volumetricflask and dilute to the mark with distilled water. Mixthe contents of the flask thoroughly and measure theabsorbance at the 410 nm wavelength used for thestandards using the blank solution as a zero reference.Dilute the sample and the blank with equal volumes ofdistilled water.

6 DETERMINATION OF CALIBRATIONFACTOR (KC)

Add Oml, 2 ml, 4 ml, 6 ml and 8 ml of KNO~workingstandard solution (1 ml = 100 g of NOJ to a series offine 5&ml volumetric flasks. To each flask, add 25 mlabsorbing solution, 10 ml distilled water and sodiumhydroxide (1 N) drop wise until thepH is between 9 and12 (about 25 to 35 drops each). Dilute to mark withdistilled water. Mix thoroughly and piyette 25 ml

aliquot of each solution into a separate porcelainevaporating dish. Beginning from evaporation stepfollow the analysis procedure as given in 5.2 until thesolution has been transferred to the 100-ml volumetricflask and dilute to mark. Measure the absorbanceof each solution at 410 nm wavelength on aspectrophotometer. Plot the absorbance of the solutionas ordinates against the concentration. A linearrelationship is obtained. Calculate the calibration factor(Kc) by taking the reciprocal of the slope of the line.

7 CALCULATION

7.1 Sample Volume Corrected to Standard Condition

Carryout the calculation as given below:

V,c= (~tilf’,td)(Vr-va) (p/Tf-P/~) =K,(v-25) (P/Tf–F’/TJ

where

Pf = final absolute pressure of flask, mm Hg;

Pi = initial absolute pressure of flask, mm Hg;

P,,d = standard absolute pressure, 760 mm Hg;

Tf = final absolute temperature of flask, K;

~ = initial absolute temperature of flask, K;

T.d = standard absolute temperature of flask,298.15 K;

V,C= sample volume at standard conditions, ml;

K, = 0.3923 K/mm Hg;

V, = volume of flask and valve, ml; and

V, =-volume of absorbing solution, 25ml.

7.2 Sample Concentration Corrected to StandardConditions

Carryout the calculations as given below:

~=(b’4b )xKcxlooox2xFl&

where

A, = absorbance of the sample;

Ab = absorbance of the blank;

C = concentration of NOXas NOZ, corrected tostandard conditions, mg/Nm3;

F = dilution factor (that is, 25/5, 25/10, etc)required only, if sample dilution was needed b

to reduce the absorbance into the range ofcalibration;

KC = spectrophotometer calibration factor; and

2 = 50125 the aliquot factor.

NOTE— If other than 25 ml aiiqucit is usedfor analysis. the factor 2 must be replaced bycorresponding factor.

4

1S.11255 (Part 7) :2005

ANN-EX A

(F’orewod)

COMMITTEE COMPOSITION

Environment Protection and Waste Management Sectional Committee, CHD 32

Organization

In personal cxapacity(40/14, C.R. Park, New Delhi 110019)

Bhabha Atomic Research Centre, Mumbai

Bharat Heavy Electrical Limited, Hardwar

Cement Manufacturers’ Association, New Delhi

Central Fuel Research Institute, Dhanbad

Central Leather Research Institute, Chennai

Central Mining Research Institute, Dhanbad

Central Pollution Control Board, New Delhi

Confederation of Indian Industries (CII), New Delhi

Crop Care Federation of India, New Delhi

Department of Civil Engineering, Indian Institute of Technology,New Delhi

Department of Science & Technology (TIFAC), New Delhi

Delhi College of Engineering, Delhi

Directorate General Factory Advice Service and Labour Institute,Mumbai

Directorate General .of Health Services, New Delhi

Engineers India Limited, New Delhi

Envirotech Instmments Private Limited, New Delhi

Food Research and Analysis Centre, New Delhi

Gujarat Pollution Control Board, Ahmedabad

Hindustan Lever Limited, Mumbai

Indian Chemical Manufacturers’ Association, Mumbai

Indian Council of Agricultural Research, New Delhi

Indian Council of Medical Research, New Delhi

Indian Institute of Packaging, Mumbai

Indian Oil Corporation Limited, Faridabad

[PCL, Vadodara

Industrial Toxicology Research Centre, Lucknow

Ministry of Defence (R&D), DRDO, New Delhi

Representative(s)

PROF DILIP BISWAS (Chairman)

DR V. D. PURAMK

DR T. N. MAHADEVEN(Alternate)

DR N. G. SHRIVASTAVA

DR K. C. NARANG

DR GULAB SINGH

DR L. C. RAM (Alternate)

DR S. RAJAMANI

DR B. K. TEWARY ,

DR S. D. MAXHIJANI

DR C. S. SHARMA(Alternate 1)DR S. K. TYAGI (Alternate II)

SHRI A. K. GHOSE

SHRI R. P. SHARMA(Alternate)

SHIUP. N. PARMESHAWARAN

DR MUKESHKHARE

DR ATUL MITTAL (Alternate I)DR ARVINDNEMA (Alternate 11)

DR P. SANJEEVARAO

DR G. SIUNJVASAN(Alternate)

SHRI RAKESH“MEHROFRA

Smu V. K. MINGCHA(Alternate 1)

DR (SHRJMATJ)A. MANDAL (Alternate 11)

SHRJ S. S. GAUTAM

SHJUM. R. RAJPUT(Alternate)

DR (SHRIMATI)MADHURJSHARMA

SHRJ B. B. LAL

SHJUSUSHEELSADH (Alfernafe)

SHRJ RAKESHAGARWAL

DR RAJSNORAPJWSAD(A/ternale)

DR S. K. SAXENA

DR R. PRABHAKARAN(Alternate)

KUMARJP. S. SHAH

SHRI B. B. DAVE

Ssuu ADITVA JHAVAR(Alternate)

SHRJV. N. DAS

SHRJA. A. PANJWANI(Alternate)

DR R. C. MAHESHWAJO

SHRJ‘H. N. SAIYAO

SHRJ S. C. ADAK

REPRESENTATIVE

SHRI P. VIJAYARAGHAVAN

DR J. D. DESAI (Alfernate)

DR S. .K. BNARGAVA

SHJUJ. C. KAPOOR

5

IS 11255 (Part 7): 2005

Organization

Ministry of Environment & Forests, New Delhi

Ministry of Non conventional Energy Sources, New Delhi

Town & Country Planning Organization, Ministry of UrbanDevelopment, New Delhi

Municipal Corporation of Greater Mumbai, Mumbai

National Institute of Occupational Health (ICh4R), Ahmedabad

National Environmental Engineering Research Institute, Nagpur

National Productivity Council, New Delhi

National Thermal Power Corporation Limited, New Delhi

NCCBM, New Delhi

Reliance Industries Limited, Mumbai

Shrirarn Institute of Industrial Research, New Delhi

SGS India Limited, Chermai

Steel Authority ofhrdia Limited, New Delhi

Thapar Centre for Industrial Research & Development, Patiala

The Fertilizer Association of lndia, New Delhi

BIS Directorate .General

Representative(s)

RsP5Es13NT,4TIvE

SHRIVINODKUMAR JAiN

SHIUK. K. JOAODERDR SANTOSHVLDYAOHARAN(Alternate)

DEPUTYCrrv ENGINEERCWIL(ENVT)DEPUTYEXECUTIVEENGINEER

(EMiSSIONIWENTDRYGROUP)(Alternate)

DRV. KRISHNAMURTHYDRA. K. MuWrsruEE(Alternate)

DR V. 1. PANDITDRTAPANNANDY (Alternate)

SHR.R. C. MONGADRA. K. SAXENA(Alternate)

SHRIR. GOPAL

SHRIM. S. BHAGWATDR S. N. PATI(A/terrrafe)

REPRESENTATIVE

SHRSV. G. K. NAiRDR JAGDISHKUMAR(Alfernate)

SHRI S. RAW

SHRIJ. KUMARDR MEENAKSHIKAKKAR(Alternate)

DR MAHESHWARROYDR S, K. CHAKRABORTY(Alternate)

DR (SHRIMATI)B. SWAMINATHANDR S. NAND(A/fernate)

DR U. C. SRWASTAVA,Director & Head (CHD)[Representing Director General (Ex-oficio A4errrber)]

Member SecretarySHRIN. K. PAL

Director (Chemical), BIS

6

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Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewedperiodically; a standard along with amendments is reaffirmed when such review indicates that no changes areneeded; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standardsshould ascertain that they are in possession of the latest amendments or edition by.referring.to the latest issue of‘BIS Catalogue’ and ‘Standards : Monthly Additions’.

This Indian Standard has been developed from Doc : No. CHD32(1109),

Amendments Issued SirrcePublication

Amend No. Date of Issue Text Affected

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